CN108043457B - High conductivity graphene-eosin Y composite aerogel photochemical catalyst preparation method - Google Patents
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- 239000004964 aerogel Substances 0.000 title claims abstract description 34
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000003054 catalyst Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 45
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 39
- SEACYXSIPDVVMV-UHFFFAOYSA-L eosin Y Chemical compound [Na+].[Na+].[O-]C(=O)C1=CC=CC=C1C1=C2C=C(Br)C(=O)C(Br)=C2OC2=C(Br)C([O-])=C(Br)C=C21 SEACYXSIPDVVMV-UHFFFAOYSA-L 0.000 claims abstract description 15
- 230000001699 photocatalysis Effects 0.000 claims abstract description 13
- 238000010531 catalytic reduction reaction Methods 0.000 claims abstract description 5
- 239000007791 liquid phase Substances 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 13
- 239000006185 dispersion Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 238000001816 cooling Methods 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 6
- 238000009777 vacuum freeze-drying Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 229910002804 graphite Inorganic materials 0.000 claims description 4
- 239000010439 graphite Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 239000000654 additive Substances 0.000 claims 2
- 230000000996 additive effect Effects 0.000 claims 2
- 238000001027 hydrothermal synthesis Methods 0.000 claims 2
- 239000003344 environmental pollutant Substances 0.000 claims 1
- 231100000719 pollutant Toxicity 0.000 claims 1
- 238000005286 illumination Methods 0.000 abstract description 6
- 239000011941 photocatalyst Substances 0.000 abstract description 6
- 238000004108 freeze drying Methods 0.000 abstract description 2
- LQNUZADURLCDLV-UHFFFAOYSA-N nitrobenzene Chemical compound [O-][N+](=O)C1=CC=CC=C1 LQNUZADURLCDLV-UHFFFAOYSA-N 0.000 abstract 2
- 238000010335 hydrothermal treatment Methods 0.000 abstract 1
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 12
- 238000006243 chemical reaction Methods 0.000 description 10
- 239000000243 solution Substances 0.000 description 8
- 229910052757 nitrogen Inorganic materials 0.000 description 6
- 239000000463 material Substances 0.000 description 5
- 238000007146 photocatalysis Methods 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 238000004847 absorption spectroscopy Methods 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- TYMLOMAKGOJONV-UHFFFAOYSA-N 4-nitroaniline Chemical compound NC1=CC=C([N+]([O-])=O)C=C1 TYMLOMAKGOJONV-UHFFFAOYSA-N 0.000 description 2
- 229910002567 K2S2O8 Inorganic materials 0.000 description 2
- 206010070834 Sensitisation Diseases 0.000 description 2
- 238000013019 agitation Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000000502 dialysis Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000001914 filtration Methods 0.000 description 2
- VBEGHXKAFSLLGE-UHFFFAOYSA-N n-phenylnitramide Chemical compound [O-][N+](=O)NC1=CC=CC=C1 VBEGHXKAFSLLGE-UHFFFAOYSA-N 0.000 description 2
- 238000006722 reduction reaction Methods 0.000 description 2
- 230000008313 sensitization Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000002893 slag Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 230000003413 degradative effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000000636 p-nitrophenyl group Chemical group [H]C1=C([H])C(=C([H])C([H])=C1*)[N+]([O-])=O 0.000 description 1
- 238000007540 photo-reduction reaction Methods 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/02—Catalysts comprising hydrides, coordination complexes or organic compounds containing organic compounds or metal hydrides
- B01J31/0231—Halogen-containing compounds
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- B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract
The invention discloses a kind of high conductivity graphene-eosin Y composite aerogel photochemical catalyst preparation methods.The Elicarb graphene of a certain amount of high conductivity, then hydrothermal treatment is added in the present invention in graphene oxide and eosin Y solution, and graphene-eosin Y composite aerogel photochemical catalyst of high conductivity can be obtained in freeze-drying.Under visible light illumination, graphene-eosin Y composite aerogel of high conductivity embodies more excellent photocatalytic activity in liquid phase photo catalytic reduction nitrobenzene and Cr (VI)；Operation of the present invention is simple and effective, has wide practical value and application prospect to more efficient graphene aerogel composite photo-catalyst is prepared.
Description
Technical field
The invention belongs to field of material technology, and in particular to a kind of high conductivity graphene-eosin Y composite aerogel light is urged
The preparation method of agent.
Background technique
Increasingly sharpening for environmental pollution and energy shortage problem, greatly threatens the sustainable development of human society.Dye
Material sensitization photocatalysis technology is since with not generating, secondary pollution, at low cost, less energy consumption, reaction condition is mild, operation is simple for it
The advantages that have become the hot spot of the research of people in recent years.However, up to now, the efficiency of dye sensitization photocatalytic system remains unchanged
It is lower.In addition, lower photocatalysis stability and in cyclic process catalyst it is a large amount of loss also seriously affected it in reality
Application in border.Three-dimensional grapheme aeroge relies on its unique structural advantage, and big specific surface area easily recycles and reuses
Advantage has attracted great concern.
However, the three-dimensional grapheme aeroge synthesized at this stage is prepared by predecessor of graphene oxide
's.The graphene aerogel of this method preparation inevitably remains oxygen-containing functional group and a large amount of fault of construction, this pole
The earth destroys the pi-conjugated electronic structure of graphene two dimension, reduces the electric conductivity of graphene, and then affect graphene-based multiple
The photocatalysis performance of light combination catalysis material.Therefore in order to substantially effectively utilize graphene, the electric conductivity for improving graphene becomes
It is very necessary.Therefore, the graphene aerogel composite photocatalyst material for inventing a kind of high conductivity is very necessary.
Summary of the invention
It is an object of the invention to for the graphene aerogel composite photocatalyst material electric conductivity being prepared at this stage
The defects of lower, provides a kind of graphene-eosin Y composite aerogel photochemical catalyst preparation method of high conductivity and its answers
With.Graphene-eosin Y composite aerogel photochemical catalyst of present aspect preparation has higher electric conductivity, under visible light liquid
Phase degradative reduction p-nitrophenyl and degradation Cr (VI) embody superior photocatalytic activity.
To achieve the above object, the present invention adopts the following technical scheme: Elicarb graphene is added to graphene oxide
In dispersion liquid, eosin Y is then added and is mixed evenly, then by hydrothermal reduction, high conductivity is can be obtained in freeze-drying
Graphene-eosin Y composite aerogel photochemical catalyst；Specific step is as follows:
(1) preparation of graphene oxide (GO):
By P2O5And K2S2O8It is uniformly mixed by the mass ratio of 1:1, is slowly added to the dense H of 12 mL 98%2SO4, it is heated to 80
DEG C, add graphite powder, 24 h of constant temperature；Room temperature is cooling, stirs after being diluted with water, then static；It filters, obtains filter residue；Gained filter
The dense H of 120 mL 98% is dissolved in after slag is dry2SO4In, 15 g KMnO are slowly added under magnetic agitation4, and control the temperature of reaction solution
Degree is lower than 20 DEG C, is then stirred to react 2 h at 35 DEG C~40 DEG C；250 mL water are slowly added to while stirring to be diluted
And the temperature of reaction solution is controlled lower than 50 DEG C；Add 1 L deionized water and 20 mL 30%H2O2(being added dropwise) continues to stir
It mixes, stands overnight；Filtering, filter residue is with 1:10 hydrochloric acid: deionized water is washed, centrifuge separation, and solid is collected in dialysis washing, dry,
Then the graphite oxide finally obtained in ultrasonic disperse to deionized water, obtains graphene oxide dispersion again；
(2) high conductivity graphene-eosin Y composite aerogel photochemical catalyst preparation:
Certain mass (2 ~ 4 mg) Elicarb graphene is added to 10 good mL graphite oxides of step (1) ultrasonic disperse
In alkene dispersion liquid (concentration is 3 mg/mL), the rear eosin Y that 2mg is added is mixed evenly, then 180 DEG C of 12 h of hydro-thermal, and
Cooling afterwards, washing, vacuum freeze drying obtain graphene-eosin Y composite aerogel photochemical catalyst of high conductivity.
A kind of graphene of high conductivity as described above-eosin Y composite aerogel photochemical catalyst can in wavelength > 420 nm
40 min of light-exposed lower irradiation, photo catalytic reduction paranitroanilinum and Cr (VI), the specific steps are as follows:
(1) a certain amount of deionized water, graphene-eosin Y composite aerogel photochemical catalyst of high conductivity are taken, to nitro
Aniline and triethanolamine are passed through nitrogen (60 mL/min) in reaction flask, adsorb certain time in the dark state, right
Nitroaniline reaches adsorption equilibrium in photocatalyst surface；Under nitrogen protection, illumination is carried out to above-mentioned system, every a timing
Between after take appropriate amount of fluid, after reaction, taken liquid is analyzed using ultraviolet-visible absorption spectroscopy；
(2) graphene-eosin Y composite aerogel photochemical catalyst, Cr of a certain amount of deionized water, high conductivity is taken
(VI) solution and triethanolamine are in reaction flask, and are passed through nitrogen (60 mL/min), adsorb a timing in the dark state
Between, paranitroanilinum reaches adsorption equilibrium in photocatalyst surface；Under nitrogen protection, illumination is carried out to above-mentioned system, every
Appropriate amount of fluid is taken after a certain period of time, and after reaction, taken liquid is analyzed using ultraviolet-visible absorption spectroscopy.
Remarkable advantage of the invention is:
(1) present invention can be realized by the way that a small amount of Elicarb graphene is added in graphene oxide and eosin Y solution
The electric conductivity of graphene aerogel eosin Y composite photo-catalyst is improved, this method experimental implementation is simple, before having a wide range of applications
Scape；
(2) graphene of high conductivity-eosin Y aeroge photocatalysis performance is more excellent, and it is low with preparation cost,
Simple production process, environmental-friendly, Yi Huishou and the advantages that can be recycled.
Detailed description of the invention
Fig. 1 is the SEM figure and photo in kind of 4EGR-EY composite aerogel photochemical catalyst made from embodiment 3；
Fig. 2 is the XPS figure of 4EGR-EY composite aerogel photochemical catalyst made from embodiment 3；
Fig. 3 is graphene-eosin Y composite aerogel photochemical catalyst XRD diagram；
Fig. 4 is the visible photo-reduction paranitroanilinum (A) of graphene aerogel-eosin Y composite aerogel photochemical catalyst and Cr
(VI) the active testing figure of (B)；
Fig. 5 is the resistance of 4EGR-EY composite aerogel photochemical catalyst made from GR-EY made from comparative example and embodiment 3
It is worth test value.
Specific embodiment
The content that the present invention is further illustrated by the following examples, but protection scope of the present invention is not limited to
The following example.
By P2O5And K2S2O8It is uniformly mixed by the mass ratio of 1:1, is slowly added to the dense H of 12 mL 98%2SO4, it is heated to 80
DEG C, add graphite powder, 24 h of constant temperature；Room temperature is cooling, stirs after being diluted with water, then static；It filters, obtains filter residue；Gained filter
The dense H of 120 mL 98% is dissolved in after slag is dry2SO4In, 15 g KMnO are slowly added under magnetic agitation4, and control the temperature of reaction solution
Degree is lower than 20 DEG C, is then stirred to react 2 h at 35 DEG C~40 DEG C；250 mL water are slowly added to while stirring to be diluted
And the temperature of reaction solution is controlled lower than 50 DEG C；Add 1 L deionized water and 20 mL 30%H2O2(being added dropwise) continues to stir
It mixes, stands overnight.Filtering, filter residue is with 1:10 hydrochloric acid: deionized water is washed, centrifuge separation, and solid is collected in dialysis washing, dry,
Then graphite oxide is finally obtained again in ultrasonic disperse to deionized water, obtains graphene oxide dispersion.
Comparative example
The eosin Y (EY) of 2 mg, and ultrasonic mixing is added in (concentration is 3 mg/mL) in 10mL graphene oxide dispersion
It stirs evenly, then 180 DEG C of 12 h of hydro-thermal, then cooling, washing, vacuum freeze drying obtain the compound gas of graphene-eosin Y
Gel (GR-EY aeroge) photochemical catalyst.
The Elicarb graphene (EGR) of 2 mg is added in 10 mL graphene oxide dispersions to (concentration is 3 mg/
ML), the eosin Y (EY) of 2 mg is added afterwards, and ultrasonic mixing stirs evenly, then 180 DEG C of 12 h of hydro-thermal, then cooling is washed
It washs, vacuum freeze drying obtains graphene-eosin Y composite aerogel (2EGR-EY aeroge) photochemical catalyst of high conductivity.
The Elicarb graphene (EGR) of 3 mg is added in 10 mL graphene oxide dispersions to (concentration is 3 mg/
ML), the eosin Y (EY) of 2 mg is added afterwards, and ultrasonic mixing stirs evenly, then 180 DEG C of 12 h of hydro-thermal, then cooling is washed
It washs, vacuum freeze drying obtains graphene-eosin Y composite aerogel (3EGR-EY aeroge) photochemical catalyst of high conductivity.
Embodiment 3
The Elicarb graphene (EGR) of 4 mg is added in 10 mL graphene oxide dispersions to (concentration is 3 mg/
ML), the eosin Y (EY) of 2 mg is added afterwards, and ultrasonic mixing stirs evenly, then 180 DEG C of 12 h of hydro-thermal, then cooling is washed
It washs, vacuum freeze drying obtains graphene-eosin Y composite aerogel (4EGR-EY aeroge) photochemical catalyst of high conductivity.
Application examples 1
GR-EY aeroge, 2EGR-EY aeroge, 3EGR-EY aeroge, 4EGR-EY aerogels are added respectively
It is added in the p-nitrophenyl amine aqueous solution of 4 groups of identical 60 ml, 10 ppm, then adds 60 μ L triethanolamines respectively, and
It is passed through nitrogen (60 mL/min), after room temperature secretly adsorbs 1 h, is placed under visible light (> 420 nm), takes out 3 mL every 10 min
Sample solution closes xenon source after 40 min of illumination, the solution centrifugal treating that will be taken, and obtained supernatant liquor is into one
Step is transferred in quartz colorimetric utensil, and the absorbance under the different photocatalysis times is measured on ultraviolet-visible spectrophotometer, thus
Obtain the curve graph (Fig. 3) of the photo catalytic reduction p-nitrophenyl amine aqueous solution under visible light illumination of catalyst under each period.
Application examples 2
GR-EY aeroge, 2EGR-EY aeroge, 3EGR-EY aeroge, 4EGR-EY aerogels are added respectively
It is added in Cr (VI) solution of 4 groups of identical 60 ml, 10 ppm, then adds 60 μ L triethanolamines respectively, and lead to
Enter nitrogen (60 mL/min), after room temperature secretly adsorbs 1 h, 40 min of illumination under visible light (> 420 nm) is placed in, every 10 min
After take appropriate amount of fluid, after reaction, (result such as Fig. 4) is analyzed to taken liquid using ultraviolet-visible absorption spectroscopy.
The foregoing is merely presently preferred embodiments of the present invention, all equivalent changes done according to scope of the present invention patent with
Modification, is all covered by the present invention.
Claims (3)
1. a kind of high conductivity graphene-eosin Y composite aerogel photochemical catalyst preparation method, it is characterised in that: including with
Lower step:
(1) graphene oxide is dissolved in ultrasonic disperse in deionized water, obtains graphene oxide dispersion；
(2) Elicarb graphene is added in the graphene oxide dispersion that step (1) obtains, eosin Y mixing is then added
It stirs evenly, then hydro-thermal process, then cooling, washing and vacuum freeze drying obtain the graphene-eosin Y aeroge and answer
Light combination catalyst；
In the step (2), the additive amount of Elicarb graphene is 2 ~ 4 mg, and the additive amount of eosin Y is 2 mg, graphite oxide
The volume of alkene dispersion liquid is 10 mL；The concentration of the graphene oxide dispersion is 3 mg/mL；
The technological parameter of the hydro-thermal process are as follows: hydrothermal temperature is 180 DEG C, and the hydro-thermal time is 12 h.
2. a kind of high conductivity graphene made from preparation method as described in claim 1-eosin Y composite aerogel light is urged
The application of agent, it is characterised in that: the high conductivity graphene-eosin Y composite aerogel photochemical catalyst is visible for liquid phase
Light photo catalytic reduction paranitroanilinum.
3. a kind of high conductivity graphene made from preparation method as described in claim 1-eosin Y composite aerogel light is urged
The application of agent, it is characterised in that: the high conductivity graphene-eosin Y composite aerogel photochemical catalyst is visible for liquid phase
Light photo catalytic reduction removes pollutant Cr (VI).
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